CN107804864A - A kind of preparation method of alumina hydrate powder and device used - Google Patents
A kind of preparation method of alumina hydrate powder and device used Download PDFInfo
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- CN107804864A CN107804864A CN201610814778.5A CN201610814778A CN107804864A CN 107804864 A CN107804864 A CN 107804864A CN 201610814778 A CN201610814778 A CN 201610814778A CN 107804864 A CN107804864 A CN 107804864A
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- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
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Abstract
The present invention relates to inorganic matter to synthesize field, in particular it relates to a kind of preparation method of alumina hydrate powder and device used.The preparation method of the alumina hydrate powder includes：Reaction is hydrolyzed in aluminum alkoxide and water under Elevated Gravity, obtained reactant mixture is separated to isolate aluminum hydroxide slurry phase and alcohol phase, and the aluminum hydroxide slurry is mutually dried.Described device includes supergravity reactor, phase-separating device and drying device, the charging aperture of the supergravity reactor is connected with aluminum alkoxide supply pipeline and water supplying pipe line respectively, the discharging opening of the supergravity reactor is connected with the phase-separating device, and lower floor's thing of the phase-separating device mutually exports to be connected with the drying device.According to the preparation method of alumina hydrate powder of the present invention, the entrainment of alcohol in gained hydrated alumina slurry can be substantially reduced, reduces the carbon residue in final alumina hydrate powder product.
Description
Technical field
The present invention relates to inorganic oxide synthesize field, in particular it relates to a kind of preparation method of alumina hydrate powder and
Device used.
Background technology
Aluminum alkoxide Hydrolyze method is to prepare a kind of main method of high-performance high-purity hydrogen aluminum oxide, its main work both at home and abroad
Skill flow is divided into two parts：The synthesis of aluminum alkoxide and the hydrolysis of aluminum alkoxide.Wherein the synthesis of aluminum alkoxide with metallic aluminium and
Fatty alcohol is raw material, reacts and obtains in the presence of catalyst.The hydrolysis of aluminum alkoxide be aluminum alkoxide at a certain temperature with
Water is reacted, and the hydroxyl in hydrone obtains hydrated alumina, together by the alkoxy in nucleophilic process substituted alkoxy aluminium
When discharge fatty alcohol, fatty alcohol can be reused for the synthesis of aluminum alkoxide after rectifying and dewatering.
In aluminum alkoxide Hydrolyze method prepares hydrated alumina technique, because aluminum alkoxide can be by filtering or depressurizing steaming
Removing impurity therein is evaporated, obtains the aluminum alkoxide of high-purity, and then hydrolyze and obtain the hydrated alumina of high-purity.This method obtains
To hydrated alumina in the impurity content such as silicon, iron, sodium, calcium, magnesium be generally less than 100ppm, hence it is evident that less than aluminum sulfate-inclined aluminium
Hydrated alumina prepared by the other methods such as the sour sodium precipitation method.The hydrated alumina of high-purity be widely used in reformation, isomerization,
During the refining catalytics such as hydrogenation, while for field of Environment Protection such as auto-exhaust catalyst, water purification agent, vent gas treatments.In recent years
The application field of high-purity alpha-alumina is further expanded, in emerging fields such as sapphire preparation, antistatic additive, high-performance ceramics
Using also more and more.
Compared with other prepare the technology of hydrated alumina, the process of aluminum alkoxide hydrolysis process is relative complex, needs
Substantial amounts of alcohol is handled, and alcohol is easy to carry secretly in aluminum hydroxide slurry, causes the loss of alcohol to increase, so as to increase aqua oxidation
The production cost of aluminium, therefore entrainment of the alcohol in aluminum hydroxide slurry how is reduced, the rate of recovery of alcohol is improved, is to reduce hydration oxygen
Change the production cost of aluminium, increase the key of the technological competitiveness.
The content of the invention
It is an object of the invention to provide a kind of preparation method of alumina hydrate powder and device used.
The invention provides a kind of preparation method of alumina hydrate powder, this method includes：By aluminum alkoxide and water super
Reaction is hydrolyzed under gravity environment, adults power level is 200~1500m/s2, obtained reactant mixture is carried out
It is separated to isolate aluminum hydroxide slurry phase and alcohol phase, and the aluminum hydroxide slurry is mutually dried.
Present invention also offers the device that a kind of aluminum alkoxide hydrolysis prepares hydrated alumina, it is anti-that the device includes hypergravity
Answer device, phase-separating device and drying device, the charging aperture of the supergravity reactor respectively with aluminum alkoxide supply pipeline and water
Supply pipeline connects, and the discharging opening of the supergravity reactor connects with the phase-separating device, under the phase-separating device
Layer thing mutually exports to be connected with the drying device.
The preparation method of alumina hydrate powder of the present invention, the hydrolysis of aluminum alkoxide is carried out under Elevated Gravity,
Alcohol entrainment is few in obtained aluminum hydroxide slurry, and the carbon residue of gained alumina hydrate powder is low, even particle distribution, Neng Gou great
Width reduces the production cost of the hydrated alumina of high-purity.Moreover, this method technique is simple, equipment cost is low, is adapted to extensive
Production.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Brief description of the drawings
Accompanying drawing is for providing a further understanding of the present invention, and a part for constitution instruction, with following tool
Body embodiment is used to explain the present invention together, but is not construed as limiting the invention.In the accompanying drawings：
Fig. 1 is the schematic diagram for the device that aluminum alkoxide hydrolysis provided by the invention prepares hydrated alumina；
Fig. 2 is hydrated alumina powder A prepared by embodiment 1 particle size distribution figure；
Fig. 3 is hydrated alumina powder C prepared by embodiment 3 particle size distribution figure；
Fig. 4 is hydrated alumina powder G prepared by embodiment 7 particle size distribution figure；
Fig. 5 is hydrated alumina powder I prepared by comparative example 1 particle size distribution figure；
Fig. 6 is hydrated alumina powder J prepared by comparative example 2 particle size distribution figure.
Description of reference numerals
The surge tank of 1 rotating packed bed reactor 2
The circulating pump of 3 two-phase laminated flow tower 4
The aluminum alkoxide supply pipeline of 5 delivery pump 6
The drier of 7 water supplying pipe line 8
The alcohol phase of 9 aluminum hydroxide slurry phase 10
Embodiment
The embodiment of the present invention is described in detail below.It is it should be appreciated that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to limit the invention.
The end points of disclosed scope and any value are not limited to the accurate scope or value herein, these scopes or
Value should be understood to comprising the value close to these scopes or value.For number range, between the endpoint value of each scope, respectively
It can be combined with each other between the endpoint value of individual scope and single point value, and individually between point value and obtain one or more
New number range, these number ranges should be considered as specific open herein.
The preparation method of alumina hydrate powder of the present invention includes：Aluminum alkoxide and water are entered under Elevated Gravity
Row hydrolysis, obtained reactant mixture is separated to isolate aluminum hydroxide slurry phase and alcohol phase, and by described in
Aluminum hydroxide slurry is mutually dried.
In the present invention, the hydrolysis of aluminum alkoxide is carried out under Elevated Gravity.Under Elevated Gravity, different size point
Molecule diffusion and interphase mass transfer process between son than in terrestrial gravitation off field much faster, solution-air, liquid-liquid, liquid-solid two-phase
Flowing contact is produced in porous media under the Elevated Gravity bigger by hundreds times to thousands of times than earth gravitational field, huge cuts
Shear force makes liquid crushing into nano level film, solid particle is broken into nano level fine particle, produces huge and fast
The boundary of speed renewal, two alternate mass transfer rates are made to greatly improve reaction than improving 1~3 order of magnitude in traditional tower
Speed.Therefore, by it is of the present invention using supergravity reactor come the hydrogen that is obtained to the method that aluminum alkoxide is hydrolyzed
Alcohol entrainment is few in aluminum oxide slurries, and the carbon residue of gained aluminium hydrate powder is low, even particle distribution, can be greatly reduced high-purity
The production cost of the hydrated alumina of degree.
In the preparation method of alumina hydrate powder of the present invention, the hydroxide isolated in the phase separation
The amount of the alcohol of aluminium paste liquid phase entrainment is less, usually less than 2 weight %, preferably below 1.9 weight %, such as 1.9 weight %,
1.5 weight %, 1.2 weight %, 0.8 weight %, 0.5 weight %, 0.3 weight %, 0.19 weight %, 0.09 weight % and this
Arbitrary value in the range of a little value any combination formation；And the carbon residue mass fraction of the alumina hydrate powder prepared after drying
(i.e. carbon residue) is relatively low, usually less than 0.3%, preferably less than 0.27%, for example, 0.27%, 0.23%, 0.21%,
0.16%th, 0.13%, 0.11%, 0.09%, 0.07% and these values be combined arbitrary value in the range of being formed.
In the preparation method of alumina hydrate powder of the present invention, the hypergravity is horizontal to be needed to control certain
In the range of, to ensure that the particle for reacting the hydrated alumina powder for carrying out fully obtaining, reaction is fully dispersed, while make hydration
The particle of alumina powder and the alcohol of generation are sufficiently separated.The horizontal particle point for causing hydrated alumina powder of too low hypergravity
Dissipate insufficient, the rate of recovery of alcohol is low, and when hypergravity is horizontal exceed OK range when, abundant progress to reaction and further carry
The rate of recovery of high alcohol is not significantly improved.Under preferable case, the hypergravity level is 200~1500m/s2, such as
200m/s2、220m/s2、300m/s2、391m/s2、612m/s2、882m/s2、1200m/s2、1378m/s2、1500m/s2And this
Arbitrary value in the range of a little value any combination formation.It is highly preferred that it is preferably 200~1400m/s that the hypergravity is horizontal2。
In the preparation method of alumina hydrate powder of the present invention, the hydrolysis of the aluminum alkoxide is in hypergravity
Reactor (such as rotating packed bed reactor) is middle to be carried out, and the centrifugation caused by rotor rotation in rotating packed bed reactor adds
The size of speed come represent hypergravity level.The rotor speed of the rotating packed bed reactor can be 300~
2000rpm, preferably 600~1500rpm.
The horizontal g of hypergravityrCalculated by lower formula (I)：
In formula (I), ω is angular speed, and unit rad/s, r are mean radius, unit m；N is rotor speed, unit：
Rev/min, r1For rotor internal diameter, unit m, r2For rotor diameter, unit m, g is controlledrFor 200~1500m/s2。
In the present invention, the rotating packed bed reactor can be selected from the high-gravity rotating bed reaction of RPB
Device, deflection type overgravity rotary bed reactor, helical duct rotating packed bed reactor, fixed-rotor are high-gravity rotating bed anti-
Device or rotating compact disc formula rotating packed bed reactor are answered, preferably packed bed rotating packed bed reactor or fixed-rotor surpasses
Gravity rotary drill reactor.
In the preparation method of alumina hydrate powder of the present invention, it is preferable that aluminum alkoxide and water cocurrent are added to
In the rotating packed bed reactor.The mass ratio of aluminum alkoxide and water can be 1：0.1-10, preferably 1：0.3-6.
In the preparation method of alumina hydrate powder of the present invention, the temperature of the hydrolysis can be 0-100
℃.When prepared alumina hydrate powder is monohydrate alumina, reaction temperature is preferably 75-120 DEG C, more preferably 80-
100℃；When prepared alumina hydrate powder is hibbsite, reaction temperature is preferably 10-55 DEG C, more preferably
25-55℃。
In the preparation method of alumina hydrate powder of the present invention, the carbon number of the aluminum alkoxide can be 1
~10, preferably 3~8.Specifically, the aluminum alkoxide is preferably selected from aluminium isopropoxide, Tributyl aluminate, n-amyl alcohol aluminium, n-hexyl alcohol
At least one of aluminium, n-heptanol aluminium and n-octyl alcohol aluminium.
In the preparation method of alumina hydrate powder of the present invention, the process of the phase separation is real in phase separator
Apply.The phase separator can use autoclave, pot type or tower type container, preferably tower type container.The height of the phase separator/straight
Footpath ratio can be 1~20, preferably 2~10.For the ease of the conveying of aluminum hydroxide slurry, the bottom decision design of phase separator
It is preferably cone for circular arc, polygonal cone or cone.
Present invention also offers the device that a kind of aluminum alkoxide hydrolysis prepares hydrated alumina, as shown in figure 1, the device bag
Include supergravity reactor 1, phase-separating device 3 and drying device 8, the charging aperture of the supergravity reactor 1 respectively with alkoxy
Aluminium supply pipeline 6 and water supplying pipe line 7 connect, and the discharging opening of the supergravity reactor 1 connects with the phase-separating device 3,
Lower floor's thing of the phase-separating device 3 mutually exports to be connected with the drying device 8.
In said device, aluminum alkoxide is added in the supergravity reactor 1 by aluminum alkoxide supply pipeline 6, water
(such as deionized water) is added in the supergravity reactor 1 by water supplying pipe line 7, and aluminum alkoxide and water are anti-in the hypergravity
To answer and reaction is hydrolyzed in device 1, the reactant mixture obtained after reaction is entered in the phase-separating device 3 and is separated,
Aluminum hydroxide slurry phase 9 and alcohol phase 10 are isolated, aluminum hydroxide slurry is mutually mutually exported by lower floor's thing of the phase-separating device 3
Enter in the drying device 8 and be dried, so as to obtain the alumina hydrate powder of high-purity.Under preferable case, alkoxy
Aluminium and water are added in the supergravity reactor 1 by pipeline 6 and the cocurrent of pipeline 7 respectively.
In a preferred embodiment, the horizontal g of hypergravity of the rotor rotation of the supergravity reactor 1rIt is preferred that control
For 200~1400m/s2。
According to one embodiment of the present invention, as shown in figure 1, described device also includes surge tank 2, the surge tank 2
Charging aperture be connected with the discharging opening of the supergravity reactor 1, the discharging opening of the surge tank 2 fills with described be separated respectively
3 charging aperture is put to connect with the charging aperture of the supergravity reactor 1.In this embodiment, in the supergravity reactor 1
Obtained reactant mixture is initially injected in the surge tank 2, and the discharging opening of the surge tank 2 is divided into two streams, one thing
Flow through to be injected in the phase separator 3 by delivery pump 5 and be separated, another burst of logistics is recycled back to described super via circulating pump 4
Gravity reactor 1.
In device of the present invention, it is high-gravity rotating bed that the supergravity reactor 1 can be selected from RPB
Reactor, deflection type overgravity rotary bed reactor, helical duct rotating packed bed reactor, fixed-rotor hypergravity rotation
Bed reactor or rotating compact disc formula rotating packed bed reactor, preferably packed bed rotating packed bed reactor or fixed-turn
Sub- rotating packed bed reactor.
In device of the present invention, the phase-separating device 3 can use autoclave, pot type or tower type container, preferably
Tower type container.The height/diameter ratio of the phase separator can be 1~20, preferably 2~10.For the ease of hydroxide aluminium paste
The conveying of liquid, the bottom of phase separator are preferably designed for circular arc, polygonal cone or cone, are preferably cone.
The present invention is further described below by embodiment, but the present invention is not limited thereto.
The entrainment of alcohol calculates with the following method in aluminum hydroxide slurry in embodiment：Take aluminum alkoxide hydrolysis gained hydrogen
Aluminum oxide slurries 100g, add deionized water and dilute aluminum hydroxide slurry to 1000g, then to the aluminum hydroxide slurry after dilution
Azeotropic distillation is carried out, when the azeotropic mixture of collection is more than 600g, is considered as and all steams the alcohol in aluminum hydroxide slurry, stops steaming
Evaporate, the alcohol content in azeotropic mixture is steamed using chromatography, calculate the quality a for steaming institute's containing alcohol in azeotropic mixture, hydroxide aluminium paste
The mass percent for carrying alcohol in liquid secretly is a%.
The carbon residue of hydrated alumina is determined using Infrared Carbon and Sulphur Determination instrument, and assay method is with reference to Yang Cuiding, Gu Kanying, Wu
What literary brightness was compiled《Petrochemical Engineering Analysis method (RIPP test methods)》The test method that middle numbering is RIPP106-90.
The Bettersize2000 that the particle diameter distribution of alumina hydrate powder is produced by hundred special Instrument Ltd. of Dandong
Type Intelligent Laser particle size analyzer determination.
Embodiment 1
By 5000g aluminium isopropoxides and 1765g deionized waters be separately heated to 50 DEG C it is standby, open high-gravity rotating bed reaction
Device, the rotor diameter of rotating packed bed reactor is 15cm, and internal diameter 5cm, regulation rotating speed is 600rpm, now hypergravity water
Put down as 220m/s2.Aluminium isopropoxide and deionized water are added in rotating packed bed reactor in manner of cocurrent flow, reaction connects
Continuous to carry out, i.e. aluminium isopropoxide and deionized water is continuously added in rotating packed bed reactor, reacts obtained isopropyl alcohol and water
The mixed liquor for closing aluminum oxide is continuously drained into surge tank, is then pumped to phase separator, and phase separator is tower type container, its
Tower height degree is 800mm, a diameter of 120mm of tower, and isopropanol is extracted out at the top of phase separator, and hydrated alumina slurry is from phase separator
Bottom is extracted out, and the mass percent of its entrainment isopropanol of sampling analysis is 1.9%.Hydrated alumina slurry is by being spray-dried
Hibbsite powder A, the inlet temperature of spray-dried instrument is 220 DEG C, and outlet temperature is 100 DEG C.Analyze hibbsite
Powder A carbon residue is 0.27%, and particle diameter distribution is as shown in Figure 2.
Embodiment 2
By 5000g Tributyl aluminates and 2195g deionized waters be separately heated to 75 DEG C it is standby, open high-gravity rotating bed reaction
Device, the rotor diameter of rotating packed bed reactor is 15cm, and internal diameter 5cm, regulation rotating speed is 700rpm, now hypergravity water
Put down as 300m/s2.Tributyl aluminate and deionized water are added in rotating packed bed reactor in manner of cocurrent flow, reaction connects
Continuous to carry out, i.e. Tributyl aluminate and deionized water is continuously added in rotating packed bed reactor, reacts obtained n-butanol and water
Close aluminum oxide mixed liquor be continuously drained into surge tank, be then pumped to the identical phase separator of example 1, n-butanol from
Extracted out at the top of phase separator, hydrated alumina slurry slave phase separator bottom is extracted out, the quality of its entrainment n-butanol of sampling analysis
Percentage is 1.5%.Hydrated alumina slurry by be spray-dried monohydrate alumina and hibbsite mixed powder
Body B, the inlet temperature of spray-dried instrument is 220 DEG C, and outlet temperature is 100 DEG C.Analysis mixed powder B carbon residue is
0.23%.
Embodiment 3
By 5000g n-amyl alcohols aluminium and 6250g deionized waters be separately heated to 90 DEG C it is standby, open high-gravity rotating bed reaction
Device, the rotor diameter of rotating packed bed reactor is 15cm, and internal diameter 5cm, regulation rotating speed is 800rpm, now hypergravity water
Put down as 391m/s2.N-amyl alcohol aluminium and deionized water are added in rotating packed bed reactor in manner of cocurrent flow, reaction connects
Continuous to carry out, i.e., n-amyl alcohol aluminium and deionized water are continuously added in rotating packed bed reactor, react obtained n-amyl alcohol and water
Close aluminum oxide mixed liquor be continuously drained into surge tank, be then pumped to the identical phase separator of example 1, n-amyl alcohol from
Extracted out at the top of phase separator, hydrated alumina slurry slave phase separator bottom is extracted out, the quality of its entrainment n-amyl alcohol of sampling analysis
Percentage is 1.2%.Hydrated alumina slurry is by being spray-dried to obtain monohydrate alumina powder C, the entrance temperature of spray-dried instrument
Spend for 220 DEG C, outlet temperature is 100 DEG C.The carbon residue for analyzing monohydrate alumina powder C is 0.21%, particle diameter distribution such as Fig. 3 institutes
Show.
Embodiment 4
5000g n-hexyl alcohol aluminium is heated to 98 DEG C, 8182g deionized waters are heated to 98 DEG C of standby, unlatching hypergravity rotations
Rotated bed reactor, the rotor diameter of rotating packed bed reactor is 15cm, and internal diameter 5cm, regulation rotating speed is 1000rpm, this
When hypergravity level be 612m/s2.N-hexyl alcohol aluminium and deionized water are added to high-gravity rotating bed reaction in manner of cocurrent flow
In device, reaction is carried out continuously, i.e., n-hexyl alcohol aluminium and deionized water are continuously added in rotating packed bed reactor, react what is obtained
The mixed liquor of n-hexyl alcohol and hydrated alumina is continuously drained into surge tank, is then pumped to and is separated with the identical of example 1
Device, n-hexyl alcohol are extracted out at the top of the phase separator, and hydrated alumina slurry slave phase separator bottom is extracted out, and sampling analysis its entrainment is just
The mass percent of hexanol is 0.8%.Hydrated alumina slurry is spray-dried by being spray-dried to obtain monohydrate alumina powder D
The inlet temperature of instrument is 220 DEG C, and outlet temperature is 100 DEG C.The carbon residue for analyzing monohydrate alumina powder D is 0.16%.
Embodiment 5
5000g n-heptanols aluminium and 9680g deionized waters are heated to 90 DEG C of standby, unlatching rotating packed bed reactors,
The rotor diameter of rotating packed bed reactor is 15cm, and internal diameter 5cm, regulation rotating speed is 1200rpm, and now hypergravity is horizontal
For 882m/s2.N-heptanol aluminium and deionized water are added in rotating packed bed reactor in manner of cocurrent flow, reaction is continuous
Carry out, i.e., n-heptanol aluminium and deionized water are continuously added in rotating packed bed reactor, react obtained n-heptanol and hydration
The mixed liquor of aluminum oxide is continuously drained into surge tank, is then pumped to and the identical phase separator of example 1, n-heptanol slave phase
Extracted out at the top of separator, hydrated alumina slurry slave phase separator bottom is extracted out, the quality hundred of its entrainment n-heptanol of sampling analysis
Divide than being 0.5%.Hydrated alumina slurry is by being spray-dried to obtain monohydrate alumina powder E, the inlet temperature of spray-dried instrument
For 220 DEG C, outlet temperature is 100 DEG C.The carbon residue for analyzing thin revolving bed powder E is 0.13%.
Embodiment 6
5000g n-octyl alcohols aluminium and 13043g deionized waters are heated to 90 DEG C of standby, unlatching rotating packed bed reactors,
The rotor diameter of rotating packed bed reactor is 15cm, and internal diameter 5cm, regulation rotating speed is 1400rpm, and now hypergravity is horizontal
For 1200m/s2.N-octyl alcohol aluminium and deionized water are added in rotating packed bed reactor in manner of cocurrent flow, reaction connects
Continuous to carry out, i.e., n-octyl alcohol aluminium and deionized water are continuously added in rotating packed bed reactor, react obtained n-octyl alcohol and water
Close aluminum oxide mixed liquor be continuously drained into surge tank, be then pumped to the identical phase separator of example 1, n-octyl alcohol from
Extracted out at the top of phase separator, hydrated alumina slurry slave phase separator bottom is extracted out, the quality of its entrainment n-octyl alcohol of sampling analysis
Percentage is 0.3%.Hydrated alumina slurry is by being spray-dried to obtain monohydrate alumina powder F, the entrance temperature of spray-dried instrument
Spend for 220 DEG C, outlet temperature is 100 DEG C.The carbon residue for analyzing monohydrate alumina powder F is 0.11%.
Embodiment 7
5000g n-nonyl alcohols aluminium and 19736g deionized waters are heated to 90 DEG C of standby, unlatching rotating packed bed reactors,
The rotor diameter of rotating packed bed reactor is 15cm, and internal diameter 5cm, regulation rotating speed is 1500rpm, and now hypergravity is horizontal
For 1378m/s2.N-nonyl alcohol aluminium and deionized water are added in rotating packed bed reactor in manner of cocurrent flow, reaction connects
Continuous to carry out, i.e., n-nonyl alcohol aluminium and deionized water are continuously added in rotating packed bed reactor, react obtained n-nonyl alcohol and water
Close aluminum oxide mixed liquor be continuously drained into surge tank, be then pumped to the identical phase separator of example 1, n-nonyl alcohol from
Extracted out at the top of phase separator, hydrated alumina slurry slave phase separator bottom is extracted out, the quality of its entrainment n-nonyl alcohol of sampling analysis
Percentage is 0.19%.Hydrated alumina slurry is by being spray-dried to obtain monohydrate alumina powder G, the entrance temperature of spray-dried instrument
Spend for 220 DEG C, outlet temperature is 100 DEG C.The carbon residue for analyzing monohydrate alumina powder G is 0.09%, particle diameter distribution such as Fig. 4 institutes
Show.
Embodiment 8
5000g Decanols aluminium and 27108g deionized waters are heated to 90 DEG C of standby, unlatching rotating packed bed reactors,
The rotor diameter of rotating packed bed reactor is 15cm, and internal diameter 5cm, regulation rotating speed is 1200rpm, and now hypergravity is horizontal
For 882m/s2.Decanol aluminium and deionized water are added in rotating packed bed reactor in manner of cocurrent flow, reaction is continuous
Carry out, i.e., Decanol aluminium and deionized water are continuously added in rotating packed bed reactor, react obtained Decanol and hydration
The mixed liquor of aluminum oxide is continuously drained into surge tank, is then pumped to and the identical phase separator of example 1, Decanol slave phase
Extracted out at the top of separator, hydrated alumina slurry slave phase separator bottom is extracted out, the quality hundred of its entrainment Decanol of sampling analysis
Divide than being 0.09%.Hydrated alumina slurry is by being spray-dried to obtain monohydrate alumina powder H, the inlet temperature of spray-dried instrument
For 220 DEG C, outlet temperature is 100 DEG C.The carbon residue for analyzing monohydrate alumina powder H is 0.07%.
Comparative example 1
5000g aluminium isopropoxides and 1765g deionized waters are separately heated to 50 DEG C, then cocurrent is added to stirring
Volume is in 10L tank reactor, and regulation speed of agitator is 200rpm, after aluminium isopropoxide and deionized water all add, dimension
Hold temperature 50 C to continue to react 1h, then stop stirring.Reaction product is added in phase separator and stands 30min, reaction production
Thing is layered as the isopropyl alcohol phase on upper strata and the hydrated alumina slurry phase of lower floor, and isopropyl alcohol phase slave phase separation top is extracted out, hydration
Aluminum oxide slurries phase slave phase separator bottom is extracted out, obtains hydrated alumina slurry, the quality of its entrainment isopropanol of sampling analysis
Percentage is 7.9%.Hydrated alumina slurry is by being spray-dried to obtain hibbsite powder I, the entrance temperature of spray-dried instrument
Spend for 220 DEG C, outlet temperature is 100 DEG C.The carbon residue for analyzing hibbsite powder I is 5.6%, particle diameter distribution such as Fig. 5 institutes
Show.
Comparative example 2
5000g n-hexyl alcohol aluminium is heated to 98 DEG C, 8182g deionized waters are heated to 98 DEG C of standby, then cocurrent additions
In the tank reactor for being 20L to the volume with stirring, regulation speed of agitator is 200rpm, and n-hexyl alcohol aluminium and deionized water are complete
After portion adds, maintain 98 DEG C of temperature to continue to react 1h, then stop stirring.Reaction product is added in phase separator, stood
30min, reaction product are layered as the n-hexyl alcohol phase on upper strata and the hydrated alumina slurry phase of lower floor, and n-hexyl alcohol is mutually from phase separator
Top is extracted out, and hydrated alumina slurry phase slave phase separator bottom is extracted out, is remained just in sampling analysis hydrated alumina slurry phase
The mass percent of hexanol is 3.5%.Hydrated alumina slurry is spray-dried by being spray-dried to obtain monohydrate alumina powder J
The inlet temperature of instrument is 220 DEG C, and outlet temperature is 100 DEG C.The carbon residue for analyzing monohydrate alumina powder J is 1.49%, particle diameter
Distribution is as shown in Figure 6.
Comparative example 3
By 5000g n-octyl alcohols aluminium and 13043g deionized waters be heated to 90 DEG C it is standby, then cocurrent be added to stirring
Volume be in 20L tank reactor, regulation speed of agitator be 200rpm, after n-octyl alcohol aluminium and the whole additions of deionized water,
Maintain 90 DEG C of temperature to continue to react 1h, then stop stirring.Reaction product is added in phase separator, stands 30min, reaction
Product is layered as the n-octyl alcohol phase on upper strata and the hydrated alumina slurry phase of lower floor, and n-octyl alcohol is mutually extracted out at the top of phase separator,
Hydrated alumina slurry phase slave phase separator bottom is extracted out, and the quality of n-octyl alcohol is remained in sampling analysis hydrated alumina slurry phase
Percentage is 3.7%.Hydrated alumina slurry is by being spray-dried to obtain monohydrate alumina powder K, the entrance temperature of spray-dried instrument
Spend for 220 DEG C, outlet temperature is 100 DEG C.The carbon residue for analyzing monohydrate alumina powder K is 1.57%.
According to the preparation method of alumina hydrate powder of the present invention it can be seen from above-described embodiment and comparative example,
The entrainment of alcohol in gained hydrated alumina slurry can be substantially reduced, reduces the carbon residue in final alumina hydrate powder product
Value, this is not only able to the quality for improving high purity hydrous alumina product, while can reduce the cost of production process, and increase should
The market competitiveness of technique.
Obviously, the above embodiment of the present invention is used for the purpose of clearly demonstrating the core concept of the present invention, and is not pair
The restriction of embodiment of the present invention, for those of ordinary skill in the art, it can make on the basis of the above description
Other various forms of changes or variation, it is every belong to obvious method that technical scheme of the present invention amplifies out with
Scheme, it is in the row of protection scope of the present invention.
Claims (11)
1. a kind of preparation method of alumina hydrate powder, this method include：Aluminum alkoxide and water are carried out under Elevated Gravity
Hydrolysis, adults power level is 200~1500m/s2, obtained reactant mixture is separated to isolate hydrogen
Aluminum oxide slurries phase and alcohol phase, and the aluminum hydroxide slurry is mutually dried.
2. according to the method for claim 1, wherein, the amount for the alcohol carried secretly in the aluminum hydroxide slurry phase isolated is low
In 2 weight %, the carbon residue mass fraction of gained alumina hydrate powder is less than 0.3% after drying.
3. method according to claim 1 or 2, wherein, the mass ratio of aluminum alkoxide and water is 1：0.1-10, preferably 1：
0.3-6。
4. method according to claim 1 or 2, wherein, when prepared alumina hydrate powder is monohydrate alumina,
Reaction temperature is 75-120 DEG C；When prepared alumina hydrate powder is hibbsite, reaction temperature is 10-55 DEG C.
5. method according to claim 1 or 2, wherein, the hydrolysis is carried out in rotating packed bed reactor,
And aluminum alkoxide and water cocurrent are added in the rotating packed bed reactor.
6. according to the method for claim 7, wherein, the rotating packed bed reactor is selected from RPB hypergravity
Rotary drill reactor, deflection type overgravity rotary bed reactor, helical duct rotating packed bed reactor, it is fixed-rotor is overweight
Power rotary drill reactor or rotating compact disc formula rotating packed bed reactor, preferably packed bed rotating packed bed reactor or
Fixed-rotor rotating packed bed reactor.
7. a kind of aluminum alkoxide hydrolysis prepares the device of hydrated alumina, the device includes supergravity reactor (1), be separated dress
Put (3) and drying device (16), the charging aperture of the supergravity reactor (1) respectively with aluminum alkoxide supply pipeline (6) and water
Supply pipeline (7) connects, and the discharging opening of the supergravity reactor (1) connects with the phase-separating device (3), the phase separation
Lower floor's thing of device (3) mutually exports to be connected with the drying device (8).
8. device according to claim 7, wherein, CENTRIFUGAL ACCELERATING caused by the rotor rotation of the supergravity reactor (1)
The horizontal g of degree-hypergravityrCalculated by following formula：
<mrow>
<msub>
<mi>g</mi>
<mi>r</mi>
</msub>
<mo>=</mo>
<msup>
<mi>&omega;</mi>
<mn>2</mn>
</msup>
<mi>r</mi>
<mo>=</mo>
<msup>
<mrow>
<mo>(</mo>
<mfrac>
<mrow>
<mn>2</mn>
<mi>&pi;</mi>
<mi>n</mi>
</mrow>
<mn>60</mn>
</mfrac>
<mo>)</mo>
</mrow>
<mn>2</mn>
</msup>
<msqrt>
<mfrac>
<mrow>
<mo>(</mo>
<msup>
<msub>
<mi>r</mi>
<mn>1</mn>
</msub>
<mn>2</mn>
</msup>
<mo>+</mo>
<msup>
<msub>
<mi>r</mi>
<mi>2</mi>
</msub>
<mn>2</mn>
</msup>
<mo>)</mo>
</mrow>
<mn>2</mn>
</mfrac>
</msqrt>
</mrow>
In formula, ω is angular speed, and unit rad/s, r are mean radius, unit m；N is rotor speed, unit：Rev/min,
r1For rotor internal diameter, unit m, r2For rotor diameter, unit m, g is controlledrFor 200~1500m/s2。
9. the device according to claim 7 or 8, wherein, described device also includes surge tank (2), the surge tank (2)
Charging aperture is connected with the discharging opening of the supergravity reactor (1), the discharging opening of the surge tank (2) respectively with the phase separation
The charging aperture of device (3) connects with the charging aperture of the supergravity reactor (1).
10. the device according to claim 7 or 8, wherein, it is overweight that the supergravity reactor (1) is selected from RPB
Power rotary drill reactor, deflection type overgravity rotary bed reactor, helical duct rotating packed bed reactor, fixed-rotor surpass
Gravity rotary drill reactor or rotating compact disc formula rotating packed bed reactor.
11. the device according to claim 7 or 8, wherein, height and the diameter ratio of the phase-separating device (3) be 1~
20, the bottom design of the phase-separating device (3) is circular arc, polygonal cone or cone, preferred conical.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4117106A (en) * | 1977-08-01 | 1978-09-26 | Continental Oil Company | Method for producing bayerite |
| CN1994887A (en) * | 2005-12-28 | 2007-07-11 | 财团法人工业技术研究院 | Preparation method of special crystal form aluminium hydroxide crystalline grain |
| CN101024503A (en) * | 2007-02-08 | 2007-08-29 | 北京化工大学 | Method for preparing ordered mesoporous aluminium oxide |
-
2016
- 2016-09-09 CN CN201610814778.5A patent/CN107804864A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4117106A (en) * | 1977-08-01 | 1978-09-26 | Continental Oil Company | Method for producing bayerite |
| CN1994887A (en) * | 2005-12-28 | 2007-07-11 | 财团法人工业技术研究院 | Preparation method of special crystal form aluminium hydroxide crystalline grain |
| CN101024503A (en) * | 2007-02-08 | 2007-08-29 | 北京化工大学 | Method for preparing ordered mesoporous aluminium oxide |
Non-Patent Citations (1)
| Title |
|---|
| 李旺兴: "《氧化铝生产理论与工艺》", 31 December 2010, 中南大学出版社 * |
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